CN104844014B - One kind is based on SiO2Heat-protecting glass of mesopore film and preparation method thereof - Google Patents
One kind is based on SiO2Heat-protecting glass of mesopore film and preparation method thereof Download PDFInfo
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- CN104844014B CN104844014B CN201510225974.4A CN201510225974A CN104844014B CN 104844014 B CN104844014 B CN 104844014B CN 201510225974 A CN201510225974 A CN 201510225974A CN 104844014 B CN104844014 B CN 104844014B
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- mesopore film
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- 239000011521 glass Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 27
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 27
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 27
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 27
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 27
- 238000004528 spin coating Methods 0.000 claims abstract description 16
- 235000019441 ethanol Nutrition 0.000 claims abstract description 15
- 239000000758 substrate Substances 0.000 claims abstract description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 11
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 10
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 230000032683 aging Effects 0.000 claims abstract 3
- 238000003756 stirring Methods 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 5
- 239000011148 porous material Substances 0.000 abstract description 4
- 230000001737 promoting effect Effects 0.000 abstract description 2
- 239000011259 mixed solution Substances 0.000 abstract 3
- 238000000034 method Methods 0.000 description 4
- 238000000235 small-angle X-ray scattering Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000013335 mesoporous material Substances 0.000 description 3
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 3
- 239000000470 constituent Substances 0.000 description 2
- 238000000802 evaporation-induced self-assembly Methods 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
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- Surface Treatment Of Glass (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention discloses one kind to be based on SiO2The heat-protecting glass of mesopore film, the material are that have SiO on the glass substrate2Mesopore film layer, the mesoporous pore size are 2 10nm, SiO2Mesopore orbit in mesopore film layer is parallel to substrate of glass.Preparation method is to carry out following steps at normal temperatures：Mixed solution and the ageing of TEOS, ethyl alcohol and dilute hydrochloric acid is first configured, is reconfigured CTAB and the mixed solution of ethyl alcohol, above two mixed solution is mixed ageing obtains spin coating liquid, and last spin coating is obtained based on SiO2The heat-protecting glass of mesopore film.The present invention based on SiO2The heat-protecting glass of mesopore film compared with other heat-barrier materials, has better heat-proof quality, and preparation method is simple, can be realized at normal temperatures under condition of equivalent thickness, and cost is relatively low, has good application prospect and promotional value.
Description
Technical field
The present invention relates to a kind of heat-protecting glasses and preparation method thereof more particularly to one kind to be based on SiO2Mesopore film it is heat-insulated
Glass and preparation method thereof.
Background technology
In the porous material, the basic mode of heat transfer is mainly shown as：The heat transfer of solid, the heat transfer of gas,
The thermal convection current and heat radiation of gas.In mesoporous material, the thermal conductivity of solid constituent is higher than the thermal conductivity of gas, and mesoporous material
With higher porosity, solid constituent is seldom, this causes the thermal conductivity of material to substantially reduce.In various mesoporous materials, it is situated between
Hole SiO2It is ideal heat-barrier material due to relatively low etc. the advantage of nontoxic, abundant raw material, solid thermal conductance.
Prepare mesoporous SiO2Film generally use sol-gel method.Sol-gel method have it is at low cost, equipment is simple, instead
The advantages that answering process easy to control, but preparing mesoporous SiO240 ~ 60 DEG C for a long time of heated at constant temperature is usually required during film.
Invention content
The purpose of the present invention is to provide a kind of excellent in heat insulating performance and prepare simply based on SiO2Mesopore film it is heat-insulated
Glass and preparation method thereof.
The present invention based on SiO2The heat-protecting glass of mesopore film is that have SiO on the glass substrate2Mesopore film layer, institute
The mesoporous pore size stated is 2-10nm, SiO2Mesopore orbit in mesopore film layer is parallel to substrate of glass.
In above-mentioned technical proposal, the SiO2The thickness of mesopore film layer is usually 200-800nm.
It is above-mentioned to be based on SiO2The preparation method of the heat-protecting glass of mesopore film, includes the following steps：
1) by TEOS（Tetraethyl orthosilicate）, ethyl alcohol and a concentration of 0.003 mol/L dilute hydrochloric acid by volume 1:1:
0.08 mixing, stir to be uniformly mixed, then thereto add in volume be above-mentioned TEOS volumes 1/3 and a concentration of 0.55 mol/L
Dilute hydrochloric acid, after stirring evenly, be aged 2-4 hours, obtain solution A；
2) by CTAB（Cetyl trimethylammonium bromide）, it is dissolved in ethyl alcohol, the mass ratio of wherein CTAB and ethyl alcohol is
0.007-0.07:1, solution B is obtained after stirring and dissolving；
3) by solution A and solution B by volume 1:2 mixing after stirring evenly, are aged 1-7 hours, obtain spin coating liquid；
4) above-mentioned spin coating drop is added in clean substrate of glass, carries out spin coating and drying, obtained based on SiO2It is mesoporous
The heat-protecting glass of film.
The present invention based on SiO2The heat-protecting glass of mesopore film, SiO2The aperture of mesopore film layer intermediary hole is 2-
10nm, than the air molecule mean free path under room temperature（About 70 nm）It is small, it is believed that the air molecule in this class duct
In no flow regime, therefore the heat transfer of gas and thermal convection current are substantially limited so that thermal conductivity is substantially reduced.In addition, SiO2
Mesopore film layer intermediary hole duct is parallel to substrate of glass, this is but also the heat transfer perpendicular to substrate of glass direction is more obstructed
Hinder.
The present invention uses the preparation method of spin coating, utilizes evaporation induced self-assembly technique（evaporation-induced
self-assembly process）, that is, pass through the volatilization of organic solvent ethyl alcohol so that inorganic source and Surfactant CTAB
Concentration increases suddenly, occurs the orderly micella of a large amount of surfactant in system, while the rate of polycondensation also increases between inorganic source
Greatly, in a short period of time, the formation of complex liquid crystalline phase is induced, forms organic-inorganic ordered composite construction.
The beneficial effects of the present invention are：The present invention is without special device and hot conditions, and preparation method is simple, in room temperature
Under the conditions of can obtain being coated with the glass of mesoporous silicon oxide films, mesopore orbit size is 2-10 nm, even size distribution and hole
Road ordered arrangement, film thickness is minimum, but with significant heat-proof quality, compared with other heat-barrier materials, this hair under condition of equivalent thickness
It is bright based on SiO2The heat-protecting glass of mesopore film has better heat-proof quality.The present invention is simple and easy to do, and cost is relatively low, has
Good application prospect and promotional value.
Description of the drawings
Fig. 1 is the small angle X ray scattering collection of illustrative plates of heat-protecting glass made from embodiment 1.
Fig. 2 is the stereoscan photograph of heat-protecting glass made from embodiment 1.
Specific embodiment
The present invention will be further described in the following with reference to the drawings and specific embodiments.
Embodiment 1
The dilute hydrochloric acid of the TEOS of 7.5 ml, the ethyl alcohol of 7.5 ml and a concentration of 0.003 mol/L of 0.6 ml are mixed, stirring
It to being uniformly mixed, then add in the dilute hydrochloric acid of a concentration of 0.55 mol/L of 2.5 ml thereto, stirs evenly, is aged 2 hours, obtains
Solution A；The CTAB of 1.2 g is dissolved in 35 ml ethyl alcohol, solution B is obtained after stirring and dissolving.Solution B is added in solution A,
After stirring evenly, it is aged 3 hours, obtains spin coating liquid.Spin coating drop is added in clean FTO substrate of glass, with first 600 r/
The rotating speed of 4000 r/min is dried 24 hours at normal temperatures later in FTO spin-on-glass plated films after min, is obtained based on SiO2
The heat-protecting glass of mesopore film.
The small angle X ray scattering curve for the heat-protecting glass that this example obtains is as shown in Figure 1, the characteristic diffraction peak at 2.271 ° is said
It is generated in bright obtained film sample orderly mesoporous.Its index is turned to（100）Crystal face, according to Prague theorem 2dsinθ
=λ, corresponding interplanar distance value is calculatedd 100For 3.88 nm.According to mesoporous hexagonal structure,a=2d 100/30.5, obtain mesoporous
The duct cycle parameter of structureaFor 4.48 nm.Therefore, mesoporous aperture is about 4 nm.
Fig. 2 is the scanning electron microscope cross-section diagram of heat-protecting glass manufactured in the present embodiment, it can be seen that it is smooth to plate film surface,
Thickness is about 471 nm.
Transient state tablet heat resource method is used to measure the thermal conductivity of FTO substrate of glass before plated film as 1.193 W/mK, sample after plated film
The thermal conductivity of product is 1.089 W/mK, and the thermal conductivity of sample has dropped 8.72% after plated film, and heat-proof quality is significantly improved.
Embodiment 2
The dilute hydrochloric acid of the TEOS of 7.5 ml, the ethyl alcohol of 7.5 ml and a concentration of 0.003 mol/L of 0.6 ml are mixed, stirring
To being uniformly mixed, then add in the dilute hydrochloric acid of a concentration of 0.55 mol/L of 2.5 ml thereto, stir and be aged 2 hours, obtain molten
Liquid A；The CTAB of 0.2 g is dissolved in 35 ml ethyl alcohol, solution B is obtained after stirring and dissolving.Solution B is added in solution A, is stirred
It mixes uniformly, is aged 1 hour, obtains spin coating liquid.Spin coating drop is added in clean substrate of glass, after first 600 r/min
The rotating speed of 4000 r/min is dried 24 hours at normal temperatures later in spin-on-glass plated film, is obtained based on SiO2Mesopore film
Heat-protecting glass.Its SiO is obtained by transmissioning electric mirror test combination small angle X-ray scattering analysis2It is mesoporous in mesopore film layer
Aperture is 2-10nm.
Embodiment 3
The dilute hydrochloric acid of the TEOS of 7.5 ml, the ethyl alcohol of 7.5 ml and a concentration of 0.003 mol/L of 0.6 ml are mixed, stirring
It to being uniformly mixed, then add in the dilute hydrochloric acid of a concentration of 0.55 mol/L of 2.5 ml thereto, stirs evenly, is aged 4 hours, obtains
Solution A；The CTAB of 2 g is dissolved in 35 ml ethyl alcohol, solution B is obtained after stirring and dissolving.Solution B is added in solution A, is stirred
It mixes uniformly, is aged 7 hours, obtains spin coating liquid.Spin coating drop is added in clean quartz glass substrate, with first 600 r/min
The rotating speed of 4000 r/min spin coating plated film on quartz glass afterwards is dried 24 hours at normal temperatures later, is obtained based on SiO2It is situated between
The heat-protecting glass of hole film.Its SiO is obtained by transmissioning electric mirror test combination small angle X-ray scattering analysis2In mesopore film layer
Mesoporous pore size be 2-10nm.
Claims (2)
1. based on SiO2The preparation method of the heat-protecting glass of mesopore film, the heat-protecting glass are that have on the glass substrate
SiO2Mesopore film layer, the mesoporous aperture are 2-10nm, SiO2Mesopore orbit in mesopore film layer is parallel to glass base
Bottom, which is characterized in that preparation method includes the following steps：
1) by the dilute hydrochloric acid of TEOS, ethyl alcohol and a concentration of 0.003 mol/L by volume 1:1:0.08 mixing, stirring are equal to mixing
It is even, then dilute hydrochloric acid of the volume for 1/3 and a concentration of 0.55 mol/L of above-mentioned TEOS volumes is added in thereto, after stirring evenly,
Ageing 2-4 hours, obtains solution A；
2) CTAB is dissolved in ethyl alcohol, the mass ratio of wherein CTAB and ethyl alcohol is 0.007-0.07:1, it obtains after stirring and dissolving molten
Liquid B；
3) by solution A and solution B by volume 1:2 mixing after stirring evenly, are aged 1-7 hours, obtain spin coating liquid；
4) above-mentioned spin coating drop is added in clean substrate of glass, carries out spin coating and drying, obtained based on SiO2Mesopore film
Heat-protecting glass.
2. according to claim 1 be based on SiO2The preparation method of the heat-protecting glass of mesopore film, which is characterized in that described
SiO2The thickness of mesopore film layer is 200-800nm.
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| CN201510225974.4A CN104844014B (en) | 2015-05-06 | 2015-05-06 | One kind is based on SiO2Heat-protecting glass of mesopore film and preparation method thereof |
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| CN104844014B true CN104844014B (en) | 2018-06-19 |
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| CN106045330B (en) * | 2016-05-27 | 2019-02-26 | 浙江大学 | A kind of mesoporous SiO2Preparation method of film and products thereof and application |
| CN108557837B (en) * | 2018-01-23 | 2021-09-28 | 福州大学 | Preparation method of SBA-15 porous film with vertical pore channels |
| CN113142669A (en) * | 2021-05-21 | 2021-07-23 | 浙江大学 | Low-temperature cigarette smoking set heat insulation pipe |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1511785A (en) * | 2002-12-30 | 2004-07-14 | 新加坡纳米材料科技有限公司 | Silicon dioxide mesoporous material and its preparing method |
| CN101168624A (en) * | 2007-11-28 | 2008-04-30 | 四川大学 | Intelligent temperature-control functional mica nacreous pigment with multi-layer structure and preparation thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1113808C (en) * | 2001-08-14 | 2003-07-09 | 复旦大学 | Preparation method of silicon oxide nano pore molecular sieve film |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1511785A (en) * | 2002-12-30 | 2004-07-14 | 新加坡纳米材料科技有限公司 | Silicon dioxide mesoporous material and its preparing method |
| CN101168624A (en) * | 2007-11-28 | 2008-04-30 | 四川大学 | Intelligent temperature-control functional mica nacreous pigment with multi-layer structure and preparation thereof |
Non-Patent Citations (1)
| Title |
|---|
| Synthesis of oriented films mesoporous silica on mica;Hong YANG et al.;《NATURE》;19990222;第379卷;703－705页 * |
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